CN105440884B - A kind of preparation and application of aqueous epoxy resins selfreparing erosion shield - Google Patents

A kind of preparation and application of aqueous epoxy resins selfreparing erosion shield Download PDF

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Publication number
CN105440884B
CN105440884B CN201510913352.0A CN201510913352A CN105440884B CN 105440884 B CN105440884 B CN 105440884B CN 201510913352 A CN201510913352 A CN 201510913352A CN 105440884 B CN105440884 B CN 105440884B
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epoxy resins
aqueous epoxy
coating
sio
corrosion inhibiter
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CN105440884A (en
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钱备
宋祖伟
郝龙
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Qingdao Agricultural University
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28—Compounds of silicon
    • C09C1/30—Silicic acid
    • C09C1/3063—Treatment with low-molecular organic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28—Compounds of silicon
    • C09C1/30—Silicic acid
    • C09C1/3072—Treatment with macro-molecular organic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28—Compounds of silicon
    • C09C1/30—Silicic acid
    • C09C1/309—Combinations of treatments provided for in groups C09C1/3009 - C09C1/3081
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/10—Treatment with macromolecular organic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/08—Anti-corrosive paints
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
    • C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
    • C01P2004/84—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases one phase coated with the other
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives

Abstract

The present invention devises a kind of aqueous epoxy resins selfreparing erosion shield, belongs to anti-corrosive metal coating field.It is characterized in that：Using the method for layer assembly by polyelectrolyte and corrosion inhibiter alternating deposit in water-based nano silicon dioxide material surface, by the nanometer silicon dioxide material centrifugation for coating polyelectrolyte and corrosion inhibiter layer by layer, washing, dry, obtain loading the nanometer silicon dioxide material of corrosion inhibiter, the nanometer silicon dioxide material for loading corrosion inhibiter is mixed according to a certain percentage with aqueous epoxy resins, curing agent, dispersant, ultrasonic wave disperses, and forms finely dispersed aqueous epoxy resins corrosion-inhibiting coating.There is good corrosion protection to carbon steel using aqueous epoxy resins coating produced by the present invention; in coating damage microcell; the nano silicon of load corrosion inhibiter can discharge inhibitor molecular absorption and form diaphragm in metal surface, play certain self-repair function.

Description

A kind of preparation and application of aqueous epoxy resins selfreparing erosion shield
Technical field
The invention belongs to anti-corrosive metal coating, and in particular to a kind of system of aqueous epoxy resins selfreparing erosion shield It is standby.
Background technology
Metal erosion can reduce the intensity of metal material, shorten the service life of hardware, and research and development is effective Corrosion protection steps have great importance.Anti-corrosive metal coating is a kind of most widely used process for corrosion control, and coating exists Aging can occur during long-term use, coat inside forms micro-crack, as micro-crack further expands and extends, coating meeting Generation bubbling and peeling, ultimately result in coating failure.In recent years, exploitation " coating with self-reparing capability " turns into anti-corrosion of metal The study hotspot of coatings art.
At present, developing the main method of coatings has three kinds：（1）Consolidant or corrosion inhibiter are encapsulated in micro-nano meter ruler The macromolecule of degree（Urea-formaldehyde, carbamide, polyurethane, polystyrene etc.）In spherical shell, painting is then dispersed in In layer.During coating breaks down, the consolidant being encapsulated in micro-nano ball flows out, and the solidification again to coating plays crosslinked action；Inhibition Agent is flowed out, and the exposed metallic matrix in corrosive medium is played a protective role.（2）Consolidant or corrosion inhibiter, which are encapsulated in, to be had The material of micro-vascular structures（Cellulose, glass fibre）In, then micro-vascular structures material is evenly spread in coating, formed Self-healing coating system with biomimetic features.During coating breaks down, consolidant or corrosion inhibiter are along micro-vascular structures passage to broken Microcell movement is split, plays healing rupture coating, protects the effect of metallic matrix.（3）Using (layer by layer) layer by layer certainly The method of assembling, polyelectrolyte is sequentially deposited at nano material（SiO2、ZnO、TiO2、CeO2、CaCO3Deng）Surface, then will Small molecule corrosion inhibiter is encapsulated in polyelectrolyte interlayer, and finally the nano material for loading corrosion inhibiter is distributed in coating.Work as coating During rupture, corrosion inhibiter slowly discharges from polyelectrolyte interlayer, adsorbs in metal surface, makes metal avoid connecing with corrosive medium Touch, reach the effect of healing holiday.It is pointed out that the research for self-healing coating has focused largely on solvent at present Type coating system, the self-healing performance study to aqueous epoxy resins coating are seldom.
Aqueous epoxy resins coating is free of organic solvent, and non-environmental-pollution, the proportion accounted in the more corrosion-inhibiting coatings of weight is increasingly Rise, will finally substitute traditional solvent-borne epoxy coating.But the corrosion protection effect of aqueous epoxy resins coating is poor, Main cause is the poor filming performance of aqueous coating, hydrophilic radical residual and easily flash rusting etc. occurs.Therefore, water-based ring is improved The antiseptic property of oxygen resinous coat has great importance.The studies above majority is directed to solvent-based coating, and research has selfreparing The aqueous epoxy resins coating of ability has great importance.
The content of the invention
The purpose of the present invention is to improve the antiseptic property of aqueous epoxy resins, there is provided a kind of aqueous epoxy resins selfreparing is prevented The preparation method of corrosion resistant coating, aqueous epoxy resins coating prepared by this method have the characteristics that green, preparation technology is simple, It can be widely applied to the metal anti-corrosive paint such as shipping industry and Nuclear Power Industry field.
To achieve the above object, the technical solution adopted by the present invention is：
A kind of preparation method of aqueous epoxy resins selfreparing erosion shield, it includes：
The first step：By the water nano SiO that particle diameter is 20nm2With deionized water by weight 1:20~1:10 mixing, 10~30min of uniform stirring in magnetic stirring apparatus, 10~20min is then disperseed in ultrasonic disperser.
Second step：The water nano SiO for taking 20~50mL first steps to prepare2The chitosan of dispersion liquid and 1~5mg/mL （CS）5~10mL of solution is mixed, 10~20min of uniform stirring in magnetic stirring apparatus, is then disperseed in ultrasonic disperser 10~20min, 10~20min finally is separated with centrifuge, upper solution is outwelled after centrifugation, lower floor is cleaned with deionized water Grain thing, obtain coating CS SiO2Particle：SiO2/CS.Wherein water nano SiO2Particle carries elecrtonegativity, and CS is to carry positive electricity Natural polycations electrolyte.
3rd step：SiO prepared by second step2/ CS and 2~5mg/mL polyaniline sodium sulfonate（PSS）Or alginate （AG）5~10mL of the aqueous solution is mixed, 10~20min of uniform stirring in magnetic stirring apparatus, is then divided in ultrasonic disperser 10~20min is dissipated, finally 10~20min is separated with centrifuge, upper solution is outwelled after centrifugation, lower floor is cleaned with deionized water Particulate matter, PSS or AG, CS SiO are coated layer by layer2Particle：SiO2/ CS/PSS or SiO2/CS/AG.Wherein PSS and AG are Polyanion electrolyte.
4th step：SiO prepared by the 3rd step2/ CS/PSS or SiO2/ CS/AG and 1~5mg/mL octadecylamine（ODA）Water 20~40mL of solution mix, 10~20min of uniform stirring in magnetic stirring apparatus, then in ultrasonic disperser disperse 10~ 20min, 10~20min finally is separated with centrifuge, upper solution is outwelled after centrifugation, lower floor's particle is cleaned with deionized water Thing, ODA, PSS or AG and CS SiO are coated layer by layer2Particle：SiO2/ CS/PSS/ODA or SiO2/CS/AG/ODA.Wherein ODA is corrosion inhibiter, has good metal surface filming function.
5th step：SiO prepared by the 4th step2/ CS/PSS/ODA or SiO2/ CS/AG/ODA and 2~5mg/mL PSS or 5~10mL of the AG aqueous solution is mixed, 10~20min of uniform stirring in magnetic stirring apparatus, is then disperseed in ultrasonic disperser 10~20min, 10~20min finally is separated with centrifuge, upper solution is outwelled after centrifugation, lower floor is cleaned with deionized water Grain thing, ODA, PSS or AG, CS SiO are coated layer by layer2Particle：SiO2/ CS/PSS/ODA/PSS or SiO2/CS/AG/ODA/ AG。
6th step：SiO prepared by the 5th step2/ CS/PSS/ODA/PSS or SiO2/ CS/AG/ODA/AG's and 1mg/mL Octadecylamine（ODA）20~40mL of the aqueous solution is mixed, 10~20min of uniform stirring in magnetic stirring apparatus, then in ultrasonic wavelength-division Dissipate and disperse 10~20min in device, finally separate 10~20min with centrifuge, upper solution is outwelled after centrifugation, uses deionized water Lower floor's particulate matter is cleaned, is coated ODA, PSS or AG, CS SiO layer by layer2Particle：SiO2/ CS/PSS/ODA/PSS/ODA or SiO2/ CS/AG/ODA/AG/ODA, final particulate matter is put into baking oven 24h is dried at 50~60 DEG C with standby.
7th step：The SiO coated layer by layer prepared by the 6th step2Particle and aqueous epoxy resins coating（Water-base epoxy tree Fat, curing agent, dispersant are with 10：10：1 mixing）According to weight ratio with 1:20~1:10 is well mixed, and aqueous epoxy resins are made Corrosion-inhibiting coating.
The present invention is beneficial to be had technical effect that：
1. using the method for LBL self-assembly in water nano SiO2Surface encapsulation corrosion inhibiter octadecylamine, polyelectrolyte sun Ion is using the chitosan of asepsis environment-protecting, and polyelectrolyte anion is using polyaniline sodium sulfonate.
2. the Nano-meter SiO_2 of LBL self-assembly prepared by the present invention2Particle chargeding performance is good, can avoid reuniting, can The high degree of dispersion in aqueous epoxy resins coating, realize structural advantage of the nano material in coated filler.
3. the water nano SiO that the present invention uses2Particle directly can be disperseed using deionized water, reduce organic solvent Usage amount.
4. in coating damage microcell, inhibitor molecular absorption can be discharged in gold by loading the nano silicon of corrosion inhibiter Metal surface forms diaphragm, plays certain self-repair function.
5. the aqueous epoxy resins coating and plain steel binding ability prepared by the present invention are good.
Brief description of the drawings
Fig. 1 is SiO2Zeta potential distribution map；Fig. 2 is SiO2/ CS Zeta potential distribution map；Fig. 3 is SiO2/CS/ PSS Zeta potential distribution map；Fig. 4 is SiO2/ CS/PSS/ODA Zeta potential distribution map；Fig. 5 is SiO2/CS/PSS/ODA/ PSS Zeta potential distribution map；Fig. 6 is SiO2/ CS/PSS/ODA/PSS/ODA Zeta potential distribution map.
The Zeta potential of the nanometer silicon dioxide material of the layer assembly of table 1
The nano silicon of layer assembly Zeta potential（mV）
SiO2 -29.4
SiO2/CS 39.3
SiO2/CS/PSS -35.8
SiO2/CS/PSS/ODA 35.0
SiO2/CS/PSS/ODA/PSS -45.8
SiO2/CS/PSS/ODA/PSS/ODA 42.0

Claims (3)

1. a kind of preparation method of aqueous epoxy resins selfreparing erosion shield, it is characterised in that utilize LBL self-assembly skill Art prepare load corrosion inhibiter water-based nano silicon dioxide material, and by it is prepared load corrosion inhibiter water-based nano silicon dioxide Material is dispersed in aqueous epoxy resins coating；Wherein, the water-based nano silicon dioxide material preparation method of corrosion inhibiter is loaded such as Under：Aqueous Nano-meter SiO_22The aqueous solution, mix, obtain with polycation electrolyte, polyanion electrolyte and corrosion inhibitor solution The SiO coated layer by layer2Particle；Water nano SiO2Particle diameter is 20nm, water nano SiO2Contained SiO in the aqueous solution2Quality point Number is 5~10%；Polycation electrolyte solution is using the chitosan solution that concentration is 1~5mg/mL, polyanion electrolysis Matter solution is using the polyaniline sodium sulfonate or sodium alginate soln that concentration is 2~5mg/mL；Corrosion inhibitor solution using Concentration is 1~5mg/mL octadecylamine solution.
2. the preparation method of aqueous epoxy resins selfreparing erosion shield according to claim 1, it is characterised in that negative It is 1 that the nanometer silicon dioxide material of corrosion inhibiter, which is carried, with the mass ratio of aqueous epoxy resins coating:20~1:10.
3. the preparation method of aqueous epoxy resins selfreparing erosion shield according to claim 1, it is characterised in that water Property epoxy coating be made up of aqueous epoxy resins, curing agent and dispersant, its mass ratio be 20:10:1.
CN201510913352.0A 2015-12-12 2015-12-12 A kind of preparation and application of aqueous epoxy resins selfreparing erosion shield Expired - Fee Related CN105440884B (en)

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CN107201140A (en) * 2017-06-17 2017-09-26 常州福隆工控设备有限公司 A kind of self-healing coatings and preparation method thereof
CN107502133B (en) * 2017-08-11 2019-04-30 北京师范大学 The corrosion-inhibiting coating and its preparation method and application for having self-reparing capability
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